Process of separating hafnium and zirconium



' lioIDrawing'.

Patented Apr. 27, 1926.

UNITED STATES,

PATENT OFFICE.

, AN'roN E UARD vxn ARKEL AND JAN nE nnrx m: BOER, or EINDHOVEN, NETHER- LANDS, ASSIGNOBS TO N. v. PHILIPS GLoniLAurENrAnnmxn or EINDHOVEN.

PROCESS OF SEIABA'IEIN'G' HAF NIUM AN D ZIRCONIUM.

To all whom'z't may concern;

Be it known that we, ANTON-EDUARD VAN 'ARKEL and JAN HENDRIK DE Bonn, both subjects of the Queen of the Netherlands, reslding at Eindhoven, in the Province of North Brabant, in the Kingdom of the Nether lands, have invented certain new and useful Improvements in or Belating'to a Process of Separating Hafi ium and Zirconium, of which the following is a specification. I

This invention comprises a process of separating a mixture of zirconiumand hafnium compounds, and more particularly of zirconiumand hafnium halogenidesu Zirconium and hafnium or their compounds are very, similar from a chemical point of view and consequently thereiare 1 and hafniumhalogenides into a liquid state.

Thus, for example, a mixture of zirconium and hafnium chloride-has the characteristic that it cannot fuse at atmospheric pressure,

and by heat is entirely'transformed'into vapour.

According group of the periodic system are known to the elements, the'highest valence numeral of which is 5 or 6, such for example as phosphorus, arsenic, antimony or molybdenum, tungsten. I

According to the invention a certain chloride) to the invention the separation of a mixture of zirconium and hafnium Application filed Au ust 5, 1.9241 Serial 309m quantity of phosphorus pentachloride can be added to amixture of zirconiumand'hafnium chloride, whereupoh the separation of the mixture thus produced is ensuredby means of fractional distillation.

The following is an example of carrying out the process accordin to the invention. I

Two parts of the mixture of zirconium and hafnium chloride and one part of phosphorus pentachloridc are mixed together.

This mixture contains an excess of phosphorus pentaehloride, serving to convert any oxide or oxychloride) which may have been formed, into zlrcomum chloride (hafnium At about 200 whereby compounds are formed between P01 and POCl -on the one hand and the zirconium and hafnium chlorides on the.

other hand; at this temperature a little PCl such as titanium chloride, are already distilled over. Between 230 C. and 360 C. a fraction rich in hafnium is distilled over, whereas a zirconium compound with POCI is not distilledover until 360 (1., and a zirconium compound with PC] is not distilled over until 410 C.

The fraction which is rich in zirconium C. the inass is melted,

zirconium oxide or oxychlori'de (hafnium IPOCI, and if present volatile impurities ther fractional distillation and this process may be continued until a mixture containing the desired high proportion of zirconium or the desired high proportion of hafnium is obtained. 1

By treating the zirconium and hafnium compounds produced with water, the phos phate which is very diflicultly worked up is produced. However, on treating the zirconium and hafnium compounds with a base the zirconium oxide or the hafnium oxide is formed, and these oxides may serve as starting material for other desired zirconium.

or hafnium compounds.

What we claim is:

1. A process for separating a mixture of zirconium and hafnium halogenides, characterized in that at least one of the halogenides of the elements of the fifth and sixth group of the periodic system is added to the mixture, whereupon she separation of the ture thus produced is obtained byfractional mixture thus produce is obtained by fracdistillatio I tional distillation. In testimony whereof We aifix our signa- 2. A process for separating a mixture of tures,-at the city of Eindhoven; this 10th 5 zirconiumand hafnium chlorides accordday of July, 1924.

ing to claim 1, characterized in that phosphorus pentachloride is added to the mix- ANTON EDUARD VAN ARKEL.

ture, whereupon theseparation of the mix- JAN I-IENDRIK DE *BOER. 

